CN109440202B - Wet spinning vacuum freeze-drying method and drying equipment - Google Patents
Wet spinning vacuum freeze-drying method and drying equipment Download PDFInfo
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- CN109440202B CN109440202B CN201811215757.7A CN201811215757A CN109440202B CN 109440202 B CN109440202 B CN 109440202B CN 201811215757 A CN201811215757 A CN 201811215757A CN 109440202 B CN109440202 B CN 109440202B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/06—Washing or drying
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Abstract
The invention provides a wet spinning vacuum freeze drying method and drying equipment, which are characterized in that: the method comprises (1) directly putting wet spinning fiber into a vacuum drying bin for freeze-drying to make the fiber totally frozen, and then carrying out the next step; (2) And heating the plate layer, vacuumizing the plate layer to ensure that the vacuum degree in the vacuum drying bin is in the range of 10pa to 800pa, and meanwhile, controlling the temperature of the plate to be 30-120 ℃ to be more than 0 ℃ to finish drying the fiber. The feeding port and the discharging port of the vacuum drying bin are respectively arranged at two ends, the guide rail in the bin is arranged at the inner top of the bin body, two ends of the guide rail in the bin are respectively connected with the guide rail outside the bin through the pneumatic connecting device to form an annular guide rail, and the lifting wire arranging table is arranged below the guide rail outside the bin close to the feeding port of the vacuum freeze drying bin. In the wet spinning process, the industrialized fiber dehydration and drying can be carried out without pre-freezing or any organic solvent, and the continuous drying production of long fibers can be realized.
Description
Technical Field
The invention belongs to the technical field of spinning, relates to fiber drying equipment and a drying method in a wet spinning process, and particularly relates to a wet spinning vacuum freeze-drying method and drying equipment.
Background
At present, in the wet spinning production process, wet fibers subjected to water washing or purification are generally soaked in an organic solvent such as alcohol, acetone and the like, and after a certain period of time, residual liquid in the fibers is centrifuged or squeezed for dehydration, and then dried in a natural airing or drying mode. The purpose is to replace the water in the nascent fiber and to arrange the internal structure of the fiber in order to increase the strength of the fiber. But adopts the production mode of organic solvent dehydration, a large amount of organic solvents are used in the production process, the production cost is high, explosion-proof equipment is required to be adopted for production, and the production factory is also required to be a class A workshop.
When the fiber is soaked by the organic solvent, the fiber with a certain length is soaked in the solvent in batches, and the mode of manually putting in and taking out the fiber is adopted, so that the fiber production process is subjected to the processes of water washing, dehydration, primary soaking of the solvent, dehydration, secondary soaking of the solvent, dehydration, oiling, dehydration, airing or drying, and the problems of long soaking time, complex production operation, large labor consumption, increased danger in the production process due to the large use of the organic solvent and the like exist.
Conventional fiber drying methods generally adopt methods such as hot air drying, vacuum pumping, microwave drying and the like, but the phenomena of yarn doubling, low fiber strength and elongation and harder hand feeling of the dried fibers are more obvious, especially the phenomena of alginic acid fibers and chitosan fibers.
The Chinese patent (ZL 2015104720101) discloses a method for vacuum freeze-drying chitin fiber or chitosan fiber, which is characterized in that wet chitosan fiber is placed in a refrigerator to be pre-frozen and then placed in vacuum drying equipment to be dried by controlling the vacuum degree, the method requires that the wet chitosan fiber is placed in the refrigerator to be pre-frozen and then placed in a vacuum drying bin, and the fiber is transferred between two sets of equipment, so that the operation method is complex and is not suitable for industrialized mass production. In addition, the frozen solid fibers are pumped out by continuously vacuumizing in the vacuum equipment, and the frozen solid materials are not heated, so that the sublimation process is slow and the drying time is long. Moreover, none of the above patents provides improvements or designs for existing vacuum freeze drying apparatus.
The existing vacuum freeze-drying equipment is mainly used for drying food or medicines and cannot be suitable for continuous drying production of long fiber bundles; in addition, the feeding and discharging of the vacuum freeze drying equipment are the same bin gate, and the fiber before drying and the fiber after drying are in the same workshop. In a workshop where the fiber before drying is usually located, the humidity is high, and the cleanliness degree cannot meet the processing conditions of the fiber after drying. Thus, there is a need for a targeted improved design of vacuum freeze drying apparatus.
Disclosure of Invention
The invention aims at the existing problems and provides a wet spinning vacuum freeze-drying method and drying equipment, which can carry out industrialized fiber dehydration drying without prefreezing or using any organic solvent in the wet spinning process, and can realize continuous drying production of long fibers.
The invention aims at realizing the following technical scheme:
the wet spinning vacuum freeze-drying method is characterized by comprising the following process steps:
(1) Placing the wet spun fiber on a tray after washing or soaking the wet spun fiber in an oiling agent, placing the tray on a tray frame of a material vehicle, conveying the tray to a heating plate in a vacuum freeze drying bin by the material vehicle, and closing a bin gate to start freeze drying;
(2) The vacuumizing system directly starts vacuumizing, continuously vacuumizing is performed, a temperature probe of the fiber is observed, the fiber is fully frozen until the temperature is reduced to below 0 ℃, and then the next step is performed;
(3) And then heating the heating plate, continuously vacuumizing the vacuum freeze drying bin to ensure that the vacuum degree in the vacuum freeze drying bin is in a range of 10pa to 800pa, controlling the temperature of the heating plate to be 30-140 ℃, and finally observing the temperature of a temperature probe on the fiber to reach more than 0 ℃ to finish drying the fiber.
The improvement of the technical scheme is as follows: in the step (1), the fibers are long fiber bundles subjected to water washing or oiling in the wet spinning process, before entering a vacuum freeze drying bin, the long fiber bundles are not sheared, continuously arranged on trays, the placed trays are placed on a tray frame of a material vehicle, the long fiber bundles among the trays are also continuously not sheared, after the long fiber bundles are dried in the step (1) and the step (2), the material vehicle is pushed out of the vacuum freeze drying bin, one end of the dried long fiber bundles is pulled out, and the long fiber bundles are introduced into buckling cutting equipment through guide rollers, so that continuous production of the long fiber bundles is realized.
Further improvement of the technical scheme is as follows: in the step (2), when the temperature of the observation temperature probe is below minus 10 ℃, heating the heating plate, setting the plate layer temperature to be 50-120 ℃, setting the vacuum degree in the vacuum freeze drying bin to be 50-300 pa, stopping heating the heating plate when the temperature of the long fiber bundle is observed to be at least 5 ℃, opening a release valve on the vacuum freeze drying bin, and pushing the long fiber bundle out of the bin body of the vacuum freeze drying bin.
Further improvement of the technical scheme is as follows: in the step (1), a material trolley sends a tray into a vacuum freeze drying bin from a feed inlet at one end of the vacuum freeze drying bin; in the step (3), after the long fiber bundles are dried, the material trolley is pushed out from a discharge hole at the other end of the vacuum freeze drying bin.
The invention discloses equipment for the wet spinning vacuum freeze drying method, which comprises a material vehicle, an out-bin guide rail and a vacuum freeze drying bin, wherein the vacuum freeze drying bin comprises a bin body, an in-bin guide rail, a cold trap, a refrigerating system, a vacuumizing system, a temperature probe, a heating plate support and a heating plate, two ends of the bin body are respectively provided with a feed inlet and a discharge outlet, and bin doors are respectively arranged on the feed inlet and the discharge outlet.
The improvement of the technical scheme is as follows: the vacuum pumping system comprises a water ring pump and a Roots pump system, the Roots pump is arranged on the outer end of a straight pipe which is arranged on the outer wall of the vacuum freeze drying bin and is communicated with the inner cavity of the bin body, and the water ring pump is arranged on the outer end of a straight pipe which is arranged on the outer wall of the vacuum freeze drying bin and is communicated with the cold trap.
Further improvement of the technical scheme is as follows: the vacuum freeze drying bin is characterized in that a gas release valve is arranged on the bin body of the vacuum freeze drying bin, and a vacuum fine adjustment valve is added on a straight pipe which is led into the inner cavity of the vacuum freeze drying bin.
Further improvement of the technical scheme is as follows: the feeding port one end of the vacuum freeze drying bin is arranged in the spinning workshop, and the discharging port one end of the vacuum freeze drying bin is arranged in the fiber post-processing workshop.
Compared with the prior art, the invention has the following advantages and positive effects:
1. in the drying step of the wet spinning process, the invention can carry out industrialized fiber dehydration and drying without pre-freezing or any organic solvent;
2. in the drying step of the wet spinning process, continuous drying production of the long fiber bundles can be realized;
3. the invention has simple process, short flow, easy operation, lower cost, convenient mass production and great economic and social benefits;
4. the feeding port and the discharging port of the vacuum freeze drying bin are respectively arranged at two ends of the bin body, and two ends of the guide rail in the bin are respectively connected with the guide rail outside the bin through the pneumatic connecting device to form an annular guide rail, so that continuous drying production of long fibers is facilitated. The feeding port and the discharging port of the vacuum freeze drying bin can be respectively arranged in workshops with two different environmental conditions, the workshop where the discharging port is located can be a workshop with high cleanliness, the processing conditions of dried fibers can be met, the workshop where the feeding port is located can be a common workshop with low cleanliness requirement, and the actual requirements of production can be met.
Drawings
FIG. 1 is a schematic top view of a wet spinning vacuum freeze drying apparatus of the present invention;
FIG. 2 is a front view of the vacuum freeze drying chamber of the present invention with the feed port door open;
FIG. 3 is a top view of the vacuum freeze drying chamber of the present invention with the feed port door open.
In the figure, 1-a vacuum freeze drying bin; 2-in-bin track; 3-pneumatic connection means; 4-out-of-bin rails; 5-a material vehicle; 6-lifting the silk swinging table; 7. a heating plate; 8. a heating plate support; 9. a temperature probe; 10. a bin gate; 11. a cold trap; 12. roots pump; 13. a vacuum fine tuning valve; 14 water ring pump.
Description of the embodiments
The invention is described in further detail below with reference to the attached drawings and examples:
referring to fig. 1-3, an embodiment of a wet spinning vacuum freeze-drying device of the invention comprises a material vehicle 5, an out-bin guide rail 4 and a vacuum freeze-drying bin 1, wherein the vacuum freeze-drying bin 1 comprises a bin body, an in-bin guide rail 2, a cold trap 12, a refrigerating system, a vacuumizing system, a temperature probe 9, a heating plate support 8 and a heating plate 7, a feed inlet and a discharge outlet are respectively arranged at two ends of the bin body, and bin doors 10 are respectively arranged on the feed inlet and the discharge outlet.
The in-bin guide rail 2 is arranged at the inner top of the bin body of the vacuum freeze drying bin 1, two ends of the in-bin guide rail 2 are respectively positioned at a feed inlet and a discharge outlet, two ends of the in-bin guide rail 2 are respectively connected with an out-bin guide rail 4 through a pneumatic connecting device 3 to form an annular guide rail, and a lifting wire swinging table 6 is arranged below the out-bin guide rail 4 close to the feed inlet of the vacuum freeze drying bin 1. During equipment installation, the feed inlet and the discharge outlet of the vacuum freeze drying bin 1 can be respectively arranged in workshops with two different environmental conditions, the workshop where the discharge outlet is positioned can be a workshop with high cleanliness, the processing conditions of dried fibers can be met, the workshop where the feed inlet is positioned can be a common workshop with low cleanliness requirement, and the actual requirements of production can be met.
The vacuum pumping system of the vacuum freeze drying bin 1 comprises a water ring pump 14 and a Roots pump 12, wherein the Roots pump 12 is arranged on the outer end of a straight pipe which is arranged on the outer wall of the vacuum freeze drying bin 1 and is communicated with the inner cavity of the bin body, and the water ring pump 14 is arranged on the outer end of the straight pipe which is arranged on the outer wall of the vacuum freeze drying bin 1 and is communicated with the cold trap 12. The invention adopts a vacuum pumping system of a combination of a rotary vane vacuum pump and a Roots pump, and because the invention does not adopt a freeze-drying mode of pre-freezing materials, a large amount of water vapor can be pumped into the rotary vane pump when the equipment is vacuumized, and the service life of the rotary vane pump is influenced, therefore, the invention changes the vacuum pump in the traditional freeze-drying equipment into the vacuum pumping system of a system composed of the water ring pump 14 and the Roots pump 12, and can reduce the problem that the service life of the equipment is influenced because the water vapor caused by incomplete water capture of a cold trap enters the rotary vane pump in the initial freeze-drying process of the materials.
The invention arranges a release valve on the bin body of the vacuum freeze drying bin 1, and adds a vacuum fine tuning valve 13 on a straight pipe which is introduced into the inner cavity of the bin body, which aims at improving the internal heat circulation rate of the vacuum freeze drying bin 1, uniformly supplementing air into the vacuum freeze drying bin 1, increasing the air flow speed and leading the materials to be dried rapidly.
The implementation mode of the drying method of the wet spinning vacuum freeze drying equipment comprises the following process steps:
(1) The wet spun fiber is put on a tray after being washed or soaked with oil, then the tray is put on a tray frame of a material vehicle, the material vehicle is hung on an outer guide rail 4 through a pulley, a material vehicle 5 is sent into a vacuum freeze drying bin 1 through a feed inlet along the outer guide rail 4 and an inner guide rail 2 in sequence and is arranged on a heating plate, and freeze drying is started after a bin door 10 is closed;
(2) The vacuumizing system directly starts vacuumizing, continuously vacuumizing is performed, a temperature probe of the fiber is observed, the fiber is fully frozen until the temperature is reduced to below 0 ℃, and then the next step is performed;
(3) Then, heating the heating plate, and simultaneously, continuously vacuumizing the vacuum freeze drying bin 1 to ensure that the vacuum degree in the vacuum freeze drying bin 1 is in a range of 10pa to 800pa, and simultaneously, controlling the temperature of the heating plate to be 30-140 ℃, and finally, observing the temperature of the temperature probe 9 on the fiber to reach more than 0 ℃ to finish drying the fiber.
Furthermore, in the step (1), the fibers are long fiber bundles which are washed or oiled in the wet spinning process, before entering the vacuum freeze drying bin 1, the long fiber bundles are not sheared, continuously put on trays, the placed trays are placed on a tray frame of the material vehicle 5, the long fiber bundles among the trays are also continuously not sheared, after the long fiber bundles are dried in the step (1) and the step (2), the material vehicle 5 is pushed out of the vacuum freeze drying bin 1 through a bin inner guide rail 2, a pneumatic connecting device 3 and a bin outer guide rail 4 through a discharge hole, one end of the dried long fiber bundles is pulled out, and the long fiber bundles are introduced into buckling cutting equipment through guide rollers, so that continuous production of the long fiber bundles is realized.
Still further, in the step (2), when the temperature of the observation temperature probe 9 is below-10 ℃, heating the heating plate is started, the temperature of the plate layer is set to be 50-120 ℃, the vacuum degree in the vacuum freeze drying bin 1 is set to be 50-300 pa, when the temperature of the long fiber bundles is observed to be at least 5 ℃, heating of the heating plate is stopped, a deflation valve on the vacuum freeze drying bin is opened, and then the long fiber bundles are pushed out of the bin body of the vacuum freeze drying bin 1.
The following is a specific example of the drying method of the wet spinning vacuum freeze-drying device of the present invention:
example 1: after a frame of chitosan wet fiber subjected to water washing and oiling is extruded and dehydrated, the wet fiber is placed on a material vehicle 5, then the material vehicle 5 is pushed into a vacuum freeze-drying bin 1 through a bin outer track 4, the material vehicle 5 is kept on a bin inner track 2 (the water capturing capacity of vacuum freeze-drying equipment is 300kg/24 h), after a bin door 10 is closed, vacuumizing is started, heating is started when the temperature of an observation temperature probe is minus 15 ℃, the heating plate is set at 60 ℃, the vacuum degree in the vacuum freeze-drying bin 1 is set in the range of 50pa to 80pa, when the temperature of the observation material reaches 5 ℃, the heating is stopped, a deflation valve of the vacuum freeze-drying bin 1 is opened, and the fiber is pushed out of a bin body of the vacuum freeze-drying bin 1. After cooling the fiber, the water content of the sample detection fiber was 2.5%.
Example 2: after three frames of water-washed and oiled alginate wet fibers are extruded and dehydrated, the weight of the alginate wet fibers is about 230 kg, the alginate wet fibers are placed on a material vehicle 5, then the material vehicle 5 is pushed into a vacuum freeze-drying cabin 1 through a cabin outer track 4, the material vehicle 5 is kept on a cabin inner track 2 (the water capturing capacity of vacuum freeze-drying equipment is 2000kg/24 h), after a cabin door is closed, vacuumizing is started, heating is started when the temperature of an observation temperature probe 9 is minus 10 ℃, the heating plate is set at 100 ℃, the vacuum degree in the vacuum freeze-drying cabin 1 is set in the range of 100pa to 180pa, heating is stopped when the temperature of the observation material reaches 15 ℃, a deflation valve of the vacuum freeze-drying cabin 1 is opened, and the fibers are pushed out of a cabin body of the vacuum freeze-drying cabin 1. After cooling the fiber, the water content of the sample detection fiber was 1.5%.
It should be understood that the above description is not intended to limit the invention to the particular embodiments disclosed, but to limit the invention to the particular embodiments disclosed, and that various changes, modifications, additions and substitutions can be made without departing from the spirit and scope of the invention.
Claims (5)
1. The wet spinning vacuum freeze-drying method is characterized by comprising the following process steps:
(1) Placing the wet spun fiber on a tray after washing or soaking the wet spun fiber in an oiling agent, placing the tray on a tray frame of a material vehicle, conveying the tray to a heating plate in a vacuum freeze drying bin by the material vehicle, and closing a bin gate to start freeze drying;
(2) The vacuumizing system directly starts vacuumizing, continuously vacuumizing is performed, a temperature probe of the fiber is observed, the fiber is fully frozen until the temperature is reduced to below 0 ℃, and then the next step is performed;
(3) Then, heating the heating plate, and continuously vacuumizing the vacuum freeze drying bin to ensure that the vacuum degree in the vacuum freeze drying bin is in a range of 10pa to 800pa, controlling the temperature of the heating plate to be 30-140 ℃, and finally observing the temperature of a temperature probe on the fiber to reach more than 0 ℃ to finish drying the fiber;
in the step (1), the fibers are long fiber bundles subjected to water washing or oiling in the wet spinning process, before entering a vacuum freeze drying bin, the long fiber bundles are not sheared, continuously put on trays, put the placed trays on a tray frame of a material vehicle, the long fiber bundles among the trays are also continuously not sheared, after the long fiber bundles are dried in the step (1) and the step (2), the material vehicle is pushed out of the vacuum freeze drying bin, one end of the dried long fiber bundles is pulled out, and the long fiber bundles are introduced into buckling cutting equipment through guide rollers, so that continuous production of the long fiber bundles is realized;
in the step (1), a material trolley sends a tray into a vacuum freeze drying bin from a feed inlet at one end of the vacuum freeze drying bin; in the step (3), after the long fiber bundles are dried, pushing out a material vehicle from a discharge hole at the other end of the vacuum freeze drying bin; the feeding port and the discharging port of the vacuum freeze drying bin are respectively arranged in workshops with two different environmental conditions.
2. The method according to claim 1, wherein in the step (2), heating the heating plate is started when the temperature of the observation temperature probe is below-10 ℃, the plate layer temperature is set to be 50-120 ℃, the vacuum degree in the vacuum freeze-drying chamber is set to be 50-300 pa, heating of the heating plate is stopped when the temperature of the long fiber bundles is observed to be at least 5 ℃, the air release valve on the vacuum freeze-drying chamber is opened, and then the long fiber bundles are pushed out of the chamber body of the vacuum freeze-drying chamber.
3. The equipment for the wet spinning vacuum freeze-drying method according to claim 1 or 2, comprising a material vehicle, an out-bin guide rail and a vacuum freeze-drying bin, wherein the vacuum freeze-drying bin comprises a bin body, an in-bin guide rail, a cold trap, a refrigerating system, a vacuumizing system, a temperature probe, a heating plate support and a heating plate, wherein two ends of the bin body are respectively provided with a feed inlet and a discharge outlet, and bin doors are respectively arranged on the feed inlet and the discharge outlet; the feeding port one end of the vacuum freeze drying bin is arranged in the spinning workshop, and the discharging port one end of the vacuum freeze drying bin is arranged in the fiber post-processing workshop.
4. A wet spinning vacuum freeze-drying method apparatus according to claim 3 wherein the vacuum pumping system comprises a water ring pump and a roots pump system, the roots pump being disposed on the outer wall of the vacuum freeze-drying chamber at the outer end of a straight tube opening into the inner cavity of the chamber body, the water ring pump being disposed on the outer wall of the vacuum freeze-drying chamber at the outer end of a straight tube opening into the cold trap.
5. The apparatus for a wet spinning vacuum freeze-drying method according to claim 4, wherein a gas release valve is arranged on a chamber body of the vacuum freeze-drying chamber, and a vacuum fine tuning valve is added on a straight pipe which is led into an inner cavity of the vacuum freeze-drying chamber.
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| CN201811215757.7A CN109440202B (en) | 2018-10-18 | 2018-10-18 | Wet spinning vacuum freeze-drying method and drying equipment |
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| CN201811215757.7A CN109440202B (en) | 2018-10-18 | 2018-10-18 | Wet spinning vacuum freeze-drying method and drying equipment |
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| CN109440202B true CN109440202B (en) | 2023-09-08 |
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| CN113373528A (en) * | 2021-06-09 | 2021-09-10 | 温州市名达服饰有限公司 | Warm-keeping western-style trousers and warm-keeping layer thereof |
| CN115852506B (en) * | 2022-12-01 | 2023-07-07 | 温州佳远生物科技有限公司 | Drying method for wet spinning of chitosan fibers |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| FR2880105B1 (en) * | 2004-12-23 | 2007-04-20 | Cie Financiere Alcatel Sa | DEVICE AND METHOD FOR CONTROLLING THE DEHYDRATION OPERATION DURING A LYOPHILIZATION TREATMENT |
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|---|---|---|---|---|
| GB1242380A (en) * | 1969-07-23 | 1971-08-11 | Leybold Heraeus Verwaltung | Improvements in freeze-drying |
| EP1277020A1 (en) * | 2000-04-19 | 2003-01-22 | AstraZeneca AB | Method of monitoring a freeze drying process |
| CN2492815Y (en) * | 2001-08-22 | 2002-05-22 | 康景隆 | Continuous vacuum freeze drier |
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